Said Belaaouad

Etude Des Proprietes Physico-Chimiques du Cyclotriphosphate Mixte de Nickel et D'argent Hexahydrate, NiAg 4 (P 3 O 9 ) 2 ·6H 2 O

Http Dx Doi Org 10 1080 10426500214290, Oct 27, 2010

ABSTRACT We have studied the dehydration and the calcination under atmospheric pressure of cyclot... more ABSTRACT We have studied the dehydration and the calcination under atmospheric pressure of cyclotriphosphate hexahydrate of nickel and silver, NiAg 4 (P 3 O 9 ) 2 ·;6H 2 O, between 25 and 600°;C by infrared spectrometry, x-ray diffraction, thermal analyses TGA, and DTA. This study led us to the identification and the crystallographic characterization of a new phase, NiAg 4 (PO 3 ) 6 , obtained between 250 and 350°;C. NiAg 4 (PO 3 ) 6 crystallizes in the triclinic system, P m 1 , with the following unit cell parameters a = 6.100(2)Å, b = 6.783(1)Å, c = 10.764(2)Å, f = 78.66(3)°;, g = 96.85(3)°;, n = 113.36(2)°;, Z = 1, V = 401Å 3 , M(20) = 133, and F(30) = 88 (0.0017; 197). The calcination of NiAg 4 (PO 3 ) 6 , between 400 and 500°;C, leads to a mixture of long-chain polyphosphates NiAg(PO 3 ) 3 and AgPO 3 . The kinetic characteristics of the dehydration of NiAg 4 (P 3 O 9 ) 2 ·;6H 2 O were determined and discussed. The vibrational spectrum of the title compound, NiAg 4 (P 3 O 9 ) 2 ·;6H 2 O, was interpreted in the domain of the stretching vibrations of the P 3 O 9 rings, on the basis of its crystalline structure and in the light of the calculation of the normal IR frequencies of the P 3 O 9 ring with the idealized D 3h symmetry. L&#39;étude de la déshydratation et de la calcination, sous pression atmosphérique, du cyclotriphosphate de nickel tétra-argent, NiAg 4 (P 3 O 9 ) 2 ·;6H 2 O, a été effectuée, entre 25 et 600°;C, par spectrométrie IR, diffraction des rayons x, ATG, et ATD. Elle a permis l&#39;identification et la caractérisation cristallographique d&#39;une nouvelle phase, NiAg 4 (PO 3 ) 6 , obtenue entre 250 et 350°;C. NiAg 4 (PO 3 ) 6 cristallise dans le système triclinique, de groupe d&#39;espace P m 1 avec Z = 1. Les paramètres de maille sont: a = 6.100(2)Å, b = 6.783(1)Å, c = 10.764(2)Å, f = 78.66(3)°;, g = 96.85(3)°;, n = 113.36(2)°;, V = 401Å 3 et les facteurs de mérite sont: M(20) = 133, et F(30) = 88 (0.0017; 197). La calcination du composé, entre 400 et 500°;C, conduit au mélange de polyphosphates à chaînes infinies NiAg(PO 3 ) 3 et AgPO 3 . Les caractéristiques cinétiques de la déshydratation de NiAg 4 (P 3 O 9 ) 2 ·;6H 2 O ont été déterminées et discutées. Le spectre IR du sel étudié a été interprété, dans le domaine des vibrations de valence des cycles, sur la base de la structure cristalline connue de son isotype NiNa 4 (P 3 O 9 ) 2 ·;6H 2 O et de nos résultats de calcul des fréquences IR fondamentales du cycle P 3 O 9 3 m de symétrie idéale D 3h .

Chemical preparation and crystal structure of barium ammonium cyclotriphosphate dihydrate

Annales De Chimie Science Des Materiaux, 2001

ABSTRACT Chemical preparation and crystal structure are reported for a new barium ammonium cyclot... more ABSTRACT Chemical preparation and crystal structure are reported for a new barium ammonium cyclotriphosphate dihydrate, BaNH4P3O9,2H2O. This compound is monoclinic P21/n with the following unit-cell dimensions: a = 7,547(1)Å, b = 12,065(1)Å, c = 11,697(1)Å, β = 101,111(1)° and Z = 4. Its crystal structure has been determined and refined down to R = 0,036, using 1983 independent reflections.

Chemical preparation, thermal behavior and crystal structure of a new cyclotriphosphate : SrNH4P3O9.3H2O

Solid State Sciences, 2000

Ammonium and barium cyclotriphosphate monohydrate, BaNH 4 P 3 O 9 ·1H 2 O, was prepared for the f... more Ammonium and barium cyclotriphosphate monohydrate, BaNH 4 P 3 O 9 ·1H 2 O, was prepared for the first time by using Boullé's process [1] by Durif et al. who reported a complete description of the atomic arrangement. BaNH 4 P 3 O 9 ·1H 2 O is monoclinic P2 1 /n with the following unit-cell dimensions: a=11.70(1)Å, b=12.12(1)Å, c=7.559(5)Å, β=101.05(5) and Z=4. Therefore, some discrepancies appear in the literature and stimulated further investigation of this compound to conclude concerning hydration level and structure. The thermal behavior of BaNH 4 P 3 O 9 ·nH 2 O showed that this cyclotriphosphate is a dihydrate and up to now no other hydrate has been described for this salt. So, the present study reports the chemical preparation, thermal behavior and crystal structure of BaNH 4 P 3 O 9 ·2H 2 O, the first cyclotriphosphate of mixed ammonium-bivalent cations M II with a new general formula M II NH 4 P 3 O 9 ·nH 2 O. Dehydration and decomposition of such cyclotriphosphates lead generally to long-chain polyphosphates, [M II (PO 3 ) 2 ] ∞ which can be used as corrosion inhibitors . The title compound has been studied through the following techniques: X-ray diffraction, IR spectrometry and thermal analyses TGA-DTA coupled. sablanca, Maroc. b Groupe des Matériaux Inorganiques, IPCMS, UMR 7504, 23 rue du Loess, 67037 Strasbourg Cedex, France. Thermal behavior and infrared studies of NiRb 4 (. Synthesis, thermal behavior and crystal structure of SrRbP 3 O 9 ·3H

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The Impact of Formative Assessment on the Learning Process and the Unreliability of the Mark for the Summative Evaluation

by bouchra gourja and Said Belaaouad

Procedia - Social and Behavioral Sciences, 2015

Chemical preparation and crystal data for two hydrated cyclotriphosphates SrMIP3O9⋅3H2O and their corresponding anhydrous SrMIP3O9 (MI=K+ and Tl+)

Powder Diffraction, 2003

Chemical preparation, kinetics of thermal behavior and infrared studies of Pb3 (P3O9 )2 .3H2O and Cd3 (P3O9 )2 .14H2O

by Said Belaaouad and Aziz Kheireddine

Mediterranean Journal of Chemistry, 2013

Chemical preparation, thermal behavior, kinetic and IR studies are given for the cyclotriphosphat... more Chemical preparation, thermal behavior, kinetic and IR studies are given for the cyclotriphosphates Pb 3 (P 3 O 9 ) 2 .3H 2 O and Cd 3 (P 3 O 9 ) 2 .14H 2 O. The later cyclotriphosphates have never been studied except their crystallographic characterization and are stable in the conditions of temperature and pressure of our laboratory until 343K. The final products of the dehydration and calcination of Pb 3 (P 3 O 9 ) 2 .3H 2 O and Cd 3 (P 3 O 9 ) 2 .14H 2 O, under atmospheric pressure, are respectively their long chain polyphosphates, [Pb(PO 3 ) 2 ] ∞ and β[Cd(PO 3 ) 2 ] ∞ . The intermediate product of the dehydration of Cd 3 (P 3 O 9 ) 2 .14H 2 O, under atmospheric pressure, is its long chain polyphosphate form α, α[Cd(PO 3 ) 2 ]  . [Pb(PO 3 ) 2 ] ∞ and β[Cd(PO 3 ) 2 ] ∞ are stable until their melting points at respectively 946K and 1153K. Two different methods, Ozawa and KAS have been selected in order to study the kinetics of thermal behavior of the cyclotriphosphates Pb 3 (P 3 O 9 ) 2 .3H 2 O and Cd 3 (P 3 O 9 ) 2 .14H 2 O for the first time.

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CHEMICAL PREPARATION AND CRYSTAL DATA FOR TWO CONDENSED PHOSPHATES NiCs4(PO3)6 AND NiK4(P3O9)2

by Said Belaaouad and Malika Tridane

Phosphorus Research Bulletin, 2003

ABSTRACT Methods of chemical preparation and crystallographic data are reported for two new conde... more ABSTRACT Methods of chemical preparation and crystallographic data are reported for two new condensed phosphates: a polyphosphate of nickel and cesium, NiCs4(PO3)6, and a cyclotriphosphate of nickel and potassium, NiK4(P3O9)2. NiCs4(PO3)6 is rhombohedral with the following unit-cell dimensions: a=b=11.602(1) Å, c=9.078(1) Å, space group P−31c, V=1058.24(1) Å3, and Z=2. NiK4(P3O9)2 is triclinic with the following unit-cell dimensions: a=6.143(8) Å, b=6.80(1) Å, c=12.80(3) Å, α=102.8(3)°, β=89.7(2)°, γ=66.03(7)°, space group P−1, V=473.56(3) Å3, and Z=1.

Chemical preparation and crystal data for two new cyclotriphosphates MIIK4(P3O9)2 (MII=Co2+ and Mn2+)

by Said Belaaouad and Malika Tridane

Powder Diffraction, 2003

ABSTRACT Methods of chemical preparation and crystal data are reported for two new anhydrous cycl... more ABSTRACT Methods of chemical preparation and crystal data are reported for two new anhydrous cyclotriphosphates MIIK4(P3O9)2 (MII=Co2+ and Mn2+). These anhydrous cyclotriphosphates CoK4(P3O9)2 and MnK4(P3O9)2 were obtained by total dehydration of corresponding hydrated cyclotriphosphates CoK4(P3O9)2.7H2O and MnK4(P3O9)2.2H2O. CoK4(P3O9)2 is triclinic, space group P−1, Z=1 with the following unit-cell dimensions: a=6.29(3) Å, b=8.00(1)Å, c=13.05(8)Å, α=86.03(5)°, β=98.00(1)°, γ=68.11(2)°. MnK4(P3O9)2 crystallizes in the rhombohedral system, space group P−31c, Z=2 with the following unit-cell dimensions: a=b=7.337(3)Å, c=19.920(1)Å.

ChemInform Abstract: Chemical Preparation, Thermal Behavior and Crystal Structure of a New Cyclotriphosphate: SrNH4P3O9×3H2O

ChemInform, 2001

Chemical preparation and crystal data for four new condensed phosphates

Powder Diffraction, 2002

ABSTRACT Methods of chemical preparation and crystallographic data are reported for four new cond... more ABSTRACT Methods of chemical preparation and crystallographic data are reported for four new condensed phosphates: one hydrated cyclotriphosphate MnAg4(P3O9)2·6H2O and three long-chain polyphosphates: MnAg2(PO3)4, NiAg4(PO3)6 and NiNa4(PO3)6. Two of these new condensed phosphates, associated with manganese, belong to previously investigated structure types.

Chemical preparation, thermal behavior and crystal structure of a new cyclotriphosphate: SrNH4P3O9·3H2O

Solid State Sciences, 2000

ABSTRACT

Etude Des Proprietes Physico-Chimiques du Cyclotriphosphate Mixte de Nickel et D'argent Hexahydrate, NiAg 4 (P 3 O 9 ) 2 ·6H 2 O

Phosphorus, Sulfur, and Silicon and the Related Elements, 2002

ABSTRACT We have studied the dehydration and the calcination under atmospheric pressure of cyclot... more ABSTRACT We have studied the dehydration and the calcination under atmospheric pressure of cyclotriphosphate hexahydrate of nickel and silver, NiAg 4 (P 3 O 9 ) 2 ·;6H 2 O, between 25 and 600°;C by infrared spectrometry, x-ray diffraction, thermal analyses TGA, and DTA. This study led us to the identification and the crystallographic characterization of a new phase, NiAg 4 (PO 3 ) 6 , obtained between 250 and 350°;C. NiAg 4 (PO 3 ) 6 crystallizes in the triclinic system, P m 1 , with the following unit cell parameters a = 6.100(2)Å, b = 6.783(1)Å, c = 10.764(2)Å, f = 78.66(3)°;, g = 96.85(3)°;, n = 113.36(2)°;, Z = 1, V = 401Å 3 , M(20) = 133, and F(30) = 88 (0.0017; 197). The calcination of NiAg 4 (PO 3 ) 6 , between 400 and 500°;C, leads to a mixture of long-chain polyphosphates NiAg(PO 3 ) 3 and AgPO 3 . The kinetic characteristics of the dehydration of NiAg 4 (P 3 O 9 ) 2 ·;6H 2 O were determined and discussed. The vibrational spectrum of the title compound, NiAg 4 (P 3 O 9 ) 2 ·;6H 2 O, was interpreted in the domain of the stretching vibrations of the P 3 O 9 rings, on the basis of its crystalline structure and in the light of the calculation of the normal IR frequencies of the P 3 O 9 ring with the idealized D 3h symmetry. L&#39;étude de la déshydratation et de la calcination, sous pression atmosphérique, du cyclotriphosphate de nickel tétra-argent, NiAg 4 (P 3 O 9 ) 2 ·;6H 2 O, a été effectuée, entre 25 et 600°;C, par spectrométrie IR, diffraction des rayons x, ATG, et ATD. Elle a permis l&#39;identification et la caractérisation cristallographique d&#39;une nouvelle phase, NiAg 4 (PO 3 ) 6 , obtenue entre 250 et 350°;C. NiAg 4 (PO 3 ) 6 cristallise dans le système triclinique, de groupe d&#39;espace P m 1 avec Z = 1. Les paramètres de maille sont: a = 6.100(2)Å, b = 6.783(1)Å, c = 10.764(2)Å, f = 78.66(3)°;, g = 96.85(3)°;, n = 113.36(2)°;, V = 401Å 3 et les facteurs de mérite sont: M(20) = 133, et F(30) = 88 (0.0017; 197). La calcination du composé, entre 400 et 500°;C, conduit au mélange de polyphosphates à chaînes infinies NiAg(PO 3 ) 3 et AgPO 3 . Les caractéristiques cinétiques de la déshydratation de NiAg 4 (P 3 O 9 ) 2 ·;6H 2 O ont été déterminées et discutées. Le spectre IR du sel étudié a été interprété, dans le domaine des vibrations de valence des cycles, sur la base de la structure cristalline connue de son isotype NiNa 4 (P 3 O 9 ) 2 ·;6H 2 O et de nos résultats de calcul des fréquences IR fondamentales du cycle P 3 O 9 3 m de symétrie idéale D 3h .

CHEMICAL PREPARATION, THERMAL BEHAVIOR, KINETIC AND INFRARED STUDIES AND QUANTUM CHEMICAL CALCULATIONS OF Ca3(P3O9)2•10H2O

by Said Belaaouad, Mohammed Moutaabbid, and Aziz Kheireddine

Phosphorus Research Bulletin, 2007

... Said Belaaouad*, Malika Tridane, Hind Chennak, Rachid Tamani, Abdelkebir Kenz,Mohammed Moutaa... more

Chemical preparation, thermal behavior and crystal structure of ammonium barium cyclotriphosphate dihydrate

Materials Research Innovations, 2000

Ammonium and barium cyclotriphosphate monohydrate, BaNH 4 P 3 O 9 ·1H 2 O, was prepared for the f... more Ammonium and barium cyclotriphosphate monohydrate, BaNH 4 P 3 O 9 ·1H 2 O, was prepared for the first time by using Boullé's process [1] by Durif et al. who reported a complete description of the atomic arrangement. BaNH 4 P 3 O 9 ·1H 2 O is monoclinic P2 1 /n with the following unit-cell dimensions: a=11.70(1)Å, b=12.12(1)Å, c=7.559(5)Å, β=101.05(5) and Z=4. Therefore, some discrepancies appear in the literature and stimulated further investigation of this compound to conclude concerning hydration level and structure. The thermal behavior of BaNH 4 P 3 O 9 ·nH 2 O showed that this cyclotriphosphate is a dihydrate and up to now no other hydrate has been described for this salt. So, the present study reports the chemical preparation, thermal behavior and crystal structure of BaNH 4 P 3 O 9 ·2H 2 O, the first cyclotriphosphate of mixed ammonium-bivalent cations M II with a new general formula M II NH 4 P 3 O 9 ·nH 2 O. Dehydration and decomposition of such cyclotriphosphates lead generally to long-chain polyphosphates, [M II (PO 3 ) 2 ] ∞ which can be used as corrosion inhibitors . The title compound has been studied through the following techniques: X-ray diffraction, IR spectrometry and thermal analyses TGA-DTA coupled. sablanca, Maroc. b Groupe des Matériaux Inorganiques, IPCMS, UMR 7504, 23 rue du Loess, 67037 Strasbourg Cedex, France. Thermal behavior and infrared studies of NiRb 4 (. Synthesis, thermal behavior and crystal structure of SrRbP 3 O 9 ·3H

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Chemical preparation, crystallographic characterization, thermal behavior and IR studies of a new cyclotriphosphate SrTlP3O9·3H2O

by Said Belaaouad, Mohammed Moutaabbid, Hicham Moutaabbid, and Aziz Kheireddine

Materials Research Bulletin, 2002

Chemical preparation, crystallographic characterization and vibrational studies are reported for ... more Chemical preparation, crystallographic characterization and vibrational studies are reported for two new condensed phosphates associated to nickel-rubidium NiRb 4 (P 3 O 9 ) 2 and strontium-thallium SrTl 4 (P 3 O 9 ) 2 . SrTl 4 (P 3 O 9 ) 2 was prepared by the method of ion-exchange resin and NiRb 4 (P 3 O 9 ) 2 was obtained by total thermal dehydration of NiRb 4 (P 3 O 9 ) 2 .6H2O. SrTl 4 (P 3 O 9 ) 2 is rhombhoedral , Z = 2, space group P-31c, with the following unit-cell parameters : a = 7,424(1) Å, c = 20,176(2) Å and V = 2807.46(2) (Å 3 ). NiRb 4 (P 3 O 9 ) 2 is triclinic, Z = 2, space group P-1, with the following unit-cell parameters : a = 8,046(9) Å , b = 9,733(0) Å, c = 4,327(5) Å, α = 98.053°, β = 88.616°, γ = 84.761° and V = 333,95(2) (Å 3 ). Vibrational study is also reported for the title compounds.

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Chemical preparation, crystal structure, thermal behavior and IR studies of barium thallium cyclotriphosphate dihydrate

Journal of Physics and Chemistry of Solids, 2003

ABSTRACT

Chemical preparation and crystal structure of barium ammonium cyclotriphosphate dihydrate

ABSTRACT Chemical preparation and crystal structure are reported for a new barium ammonium cyclot... more ABSTRACT Chemical preparation and crystal structure are reported for a new barium ammonium cyclotriphosphate dihydrate, BaNH4P3O9,2H2O. This compound is monoclinic P21/n with the following unit-cell dimensions: a = 7,547(1)Å, b = 12,065(1)Å, c = 11,697(1)Å, β = 101,111(1)° and Z = 4. Its crystal structure has been determined and refined down to R = 0,036, using 1983 independent reflections.

STUDY OF THE STRUCTURAL MODIFICATIONS OF CYCLOPHOSPHATES OF MANGANESE FROM M3 (P3O9)2.10H2O TO Mn2P4O12 DURING THERMAL BEHAVIOR PROCESS BY INFRARED SPECTROSCOPY

by bouchra gourja, Mustafa Belhabra, and Said Belaaouad

Chemical preparation, thermal behavior, kinetic and IR studies are given for the cyclotriphosphat... more Chemical preparation, thermal behavior, kinetic and IR studies are given for the cyclotriphosphate Mn 3 (P 3 O 9) 2 .10H 2 O. Mn 3 (P 3 O 9) 2 .10H 2 O, which has already been studied, is monoclinic P2 1 /n with the following unit-cell dimensions : a = 9.631(5)Å,b = 18,173(7)Å, c = 7,976(4),  = 109,438(4)° and Z = 2. The study of the structural modifications of cyclophosphates of manganese from Mn 3 (P 3 O 9) 2 .10H 2 O to Mn 2 P 4 O 12 during thermal behavior process by infrared spectroscopy has never been performed. It's the first time where a cyclotriphosphate P 3 O 9 is converted to a cyclotetraphosphate P 4 O 12 by thermal dehydration. The thermal behavior of Mn 3 (P 3 O 9) 2 .10H 2 O has been investigated and interpreted by comparison with IR absorption spectrometry, X-ray diffraction experiments, chemical analyses, thermal analyses (TGA-DTA) and differential scanning calorimetry (DSC). Mn 3 (P 3 O 9) 2 .10H 2 O is stable, in the conditions of temperature and pressure of our laboratory, until 70°C. It is impossible to dehydrate Mn 3 (P 3 O 9) 2 .10H 2 O without breaking its rings P 3 O 9 3-and leading to amorphous compounds in X-ray diffraction and IR absorption spectrometry. The final product of the dehydration and calcination of Mn 3 (P 3 O 9) 2 .10H 2 O cyclotriphosphate, under atmospheric pressure, is its cyclotetraphosphate Mn 2 P 4 O 12. Mn 2 P 4 O 12 is prepared otherwise by dry way.

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